HRID1199675

反应详情

EQUATION

反应方程式

HRID 1199675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chlorobenzenesulphonyl chloride (1.17 g) was added portionwise to a solution of 4-(5-aminopyrid-2-yl)butanoic acid (1 g) in pyridine (15 ml). The resulting solution was allowed to stand at room temperature overnight when the solvent was removed under reduced pressure. The residue was dissolved in dilute sodium hydroxide solution (50 ml) and extracted with chloroform (4×50 ml) and the chloroform extracts were discarded. The aqueous layer was adjusted to pH=4 and was extracted with chloroform (3×100 ml). The chloroform extracts were dried over magnesium sulphate, the solvent was removed and residue was recrystallised from acetonitrile/water 1:1 to give the title compound (0.7 g) as white plates. m.p. 178°-180° C.

WORKUP

后处理

  1. customwhen the solvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in dilute sodium hydroxide solution (50 ml)
  3. extractionextracted with chloroform (4×50 ml)
  4. extractionwas extracted with chloroform (3×100 ml)
  5. dry with materialThe chloroform extracts were dried over magnesium sulphate
  6. customthe solvent was removed
  7. customresidue was recrystallised from acetonitrile/water 1:1